The simplest Methamphetamine synthesis from Amphetamine

[Wallpaper]

Amph cannot be evaporated in hot air

G.PattonCan mercuric chloride be used as Will??

 

[G.Patton]

Can mercuric chloride be used as Will??

Wallpaperyes

 

[UWe9o12jkied91d]

If you use D Amph to start with you get D meth. I was planning to try this synthesis, and I plan to use racemic amph and then resolve the meth just in case something goes wrong with a route I have never tried, then D amph would be wasted...

Is there anyone who has actually tried this synthesis in practice? I have read it in several places, but never found a practical report. Experts can you please give some reassurance?

diogenesCan you explain how you drew the conclusion it’s not gonna racemize? Actually want to know, not questioning you.

 

[diogenes]

Can you explain how you drew the conclusion it’s not gonna racemize? Actually want to know, not questioning you.

UWe9o12jkied91dI don`t take it as questioning . We are here to help each other with information. As I haven`t tried this conversion (neither from racemic nor from D-amphetamine) I can only rely on Rhodium`s notes on

Monomethylation of Amphetamines - [www.rhodium.ws]

I would just use racemic amphetamine by the way, as Methamphetamine can be resolved by the same methods as amphetamine and why risk valuable D isomer when the end results are not known.

`Formaldehyde and Aluminum Amalgam`
N-Methyl-amphetamines were prepared by the reaction of the corresponding amphetamine with formaldehyde and reduction in the absence of acid. Thus, a mixture of 1 mole amphetamine freebase (136g) and 1 mole aqueous formaldehyde (81ml 37% or 75ml 40%) in 350 ml alcohol and an excess of aluminum amalgam was reduced for several hours, water added, aluminum hydroxide filtered off, the solution acidified and evaporated, and the freebase separated by means of alkali yielding phenyl-N-methylisopropylamine, converted to the hydrochloride, mp 140°C. Similarly, 70g d-amphetamine in alcohol with aluminum and 1 mole formaldehyde gave d-methamphetamine, which was converted to the phosphate salt. 1-Phenyl-2-aminopropanol similarly yielded ephedrine.`
(Emphasis from me.)

Anyway, I still invite anyone out anyone to share his experience having actually tried this synthesis and having some real-life experience with it. I am going to try it at some point, but would have been great to know that it really works before sacrifising a lot of material and time. The other option is starting from P2NP reducing it to the imine and then hydrolysing in acidic environment to P2P, but this then involves a further amination of the P2P with methylamine which I think is excessive as there has already been one (following condensation of benzaldehyde with nitroethane). The method I would use also requires quite a lot of Acetic acid to reduce e.g. on iron catalyst then hydrolyse with the acid. If there is no one having tried this, then I will do a comparison and let the forum members know.

 

[UWe9o12jkied91d]

I don`t take it as questioning . We are here to help each other with information. As I haven`t tried this conversion (neither from racemic nor from D-amphetamine) I can only rely on Rhodium`s notes on

Monomethylation of Amphetamines - [www.rhodium.ws]

I would just use racemic amphetamine by the way, as Methamphetamine can be resolved by the same methods as amphetamine and why risk valuable D isomer when the end results are not known.

`Formaldehyde and Aluminum Amalgam`
N-Methyl-amphetamines were prepared by the reaction of the corresponding amphetamine with formaldehyde and reduction in the absence of acid. Thus, a mixture of 1 mole amphetamine freebase (136g) and 1 mole aqueous formaldehyde (81ml 37% or 75ml 40%) in 350 ml alcohol and an excess of aluminum amalgam was reduced for several hours, water added, aluminum hydroxide filtered off, the solution acidified and evaporated, and the freebase separated by means of alkali yielding phenyl-N-methylisopropylamine, converted to the hydrochloride, mp 140°C. Similarly, 70g d-amphetamine in alcohol with aluminum and 1 mole formaldehyde gave d-methamphetamine, which was converted to the phosphate salt. 1-Phenyl-2-aminopropanol similarly yielded ephedrine.`
(Emphasis from me.)

Anyway, I still invite anyone out anyone to share his experience having actually tried this synthesis and having some real-life experience with it. I am going to try it at some point, but would have been great to know that it really works before sacrifising a lot of material and time. The other option is starting from P2NP reducing it to the imine and then hydrolysing in acidic environment to P2P, but this then involves a further amination of the P2P with methylamine which I think is excessive as there has already been one (following condensation of benzaldehyde with nitroethane). The method I would use also requires quite a lot of Acetic acid to reduce e.g. on iron catalyst then hydrolyse with the acid. If there is no one having tried this, then I will do a comparison and let the forum members know.

diogenesNice, it's what we like to see dood

 

[G.Patton]

The other option is starting from P2NP reducing it to the imine and then hydrolysing in acidic environment to P2P

diogenesDon't hurry please, we'll post p2np => p2p video synthesis in couple weeks.

 

[diogenes]

Don't hurry please, we'll post p2np => p2p video synthesis in couple weeks.

G.PattonCool. I will wait then and let the experts find out the details/pitfalls. Thanks Patton

 

[WinterDust]

Hi everyone,

So it is time for me now to move forward in my progress and start looking at manufacturing Crystal Methamphetamine (ICE), I have no interest in "normal" Methamphetamines.

So let me start out with posting the step and asking my questions, I would appreciate any ones knowledgeable input.

Step:

1. You have to get 1 mole amphetamine free (1) base by addition salt of your amphetamine to 20% NaOH water solution to pH 12. Mix it for 15 min and extract amphetamine free base by DCM or petrolium ether 3 x 75 mL.
   Q: It says amphetamine free base, and then salt, does it mean freebase as in amphetamineoil or dry amphetamine, if I were to guess, it means amphetamine sulphate.
   
   
2. Prepare Al amalgam. You have to use approximately ~70 g of Al foil and 1.62 g mercury(II)nitrate (Hg(NO3)2) to make amalgam as described in following topic.
   Q: No question here
   
   
3. A mixture of 1 mole amphetamine freebase (136 g) and 1 mole aqueous formaldehyde (2) (81 mL 37% or 75 mL 40%) in 350 mL EtOH (ethanole) in 5 L round bottom flask with reflux condenser and an excess of aluminum amalgam, which was prepared in advance.
   Q: The extract from step 1 in is poured into a 5L round bottom flask, togheter with 81mL 37% aqueous formaldehyde and 350mL EtOH and the aluminium amalgam?
   
   
4. Imine (3) was reduced for approximately two hours, to keep reaction temperature below ~50-60 °C. Cooling should be applied if the reaction becomes too violent.
   Q: The reaction from step 3 is mixed with either overhead stirrer or magnetic stirrer, combined with a cooler to keep the reaction mass under 60c temperature.
   
   
5. 1 L Of cooled distilled water is added to reaction mass, aluminum hydroxide is filtered off.
   Q: We add 1L of cold water into the reaction and use a buchner funnel with filter to clear it from aluminum residues?
   
   
6. The reaction mass extracted by DCM or petrolium ether 3 x 75 mL. Extracts are treated with 20 % HCl to pH 3. Resulting water layer from filtration is alkalinized by 20% NaOH aq to pH 12 and extracted with DCM or petrolium ether 3 x 75 mL. Organic layers with methamphetamine (4) are combined, concentrated in vacuum and dried over Na2SO4 or MgSO4 anhydrous.
   Q: I don't understand this at all, it's very unclear to me.
   
   I understand that there should be two different layers here. So I guess from step 5 when we add the cold water, and filter the reaction from residues of the aluminium. It will split into two layers. One organic and the one with water, the aqueous layer.
   
   The organic layer is extracted with DCM 3 x 75mL and then treated with 20% HCl to pH3
   
   The aqueous layer (water layer) is treated with with 20% NaoH to pH 12 and then extracted with DCM 3 x 75mL.
   
   After both layers are extracted and treated they are combined, concentrated in vacuum (optional) and dried using Na2SO4.
   
   If I am not wrong, this step is where we get our Methamphetamine freebase (Meth-oil)?
   
   
7. Preparation of methamphetamine hydrochloride is carried out by bubbling of dry HCl gas via organic layer. Precipitate is filtered off by suction filtration, dried. Also, you can grow Ice methamphetamine by following methods.
   Q: I don't understand this at all, it's very unclear to me.
   
   If I am not wrong, this is the step where we crystallize the Methamphetamine freebase (Meth-oil) to Methamphetamine?
   
   I would appreciate your input and knowledge on my question.
   
   Best Regards
   
   
   PS: Would admin please make this synthesis sticky.

 

[G.Patton]

Hi everyone,

So it is time for me now to move forward in my progress and start looking at manufacturing Crystal Methamphetamine (ICE), I have no interest in "normal" Methamphetamines.

So let me start out with posting the step and asking my questions, I would appreciate any ones knowledgeable input.

Step:

1. You have to get 1 mole amphetamine free (1) base by addition salt of your amphetamine to 20% NaOH water solution to pH 12. Mix it for 15 min and extract amphetamine free base by DCM or petrolium ether 3 x 75 mL.
   Q: It says amphetamine free base, and then salt, does it mean freebase as in amphetamineoil or dry amphetamine, if I were to guess, it means amphetamine sulphate.
   
   
2. Prepare Al amalgam. You have to use approximately ~70 g of Al foil and 1.62 g mercury(II)nitrate (Hg(NO3)2) to make amalgam as described in following topic.
   Q: No question here
   
   
3. A mixture of 1 mole amphetamine freebase (136 g) and 1 mole aqueous formaldehyde (2) (81 mL 37% or 75 mL 40%) in 350 mL EtOH (ethanole) in 5 L round bottom flask with reflux condenser and an excess of aluminum amalgam, which was prepared in advance.
   Q: The extract from step 1 in is poured into a 5L round bottom flask, togheter with 81mL 37% aqueous formaldehyde and 350mL EtOH and the aluminium amalgam?
   
   
4. Imine (3) was reduced for approximately two hours, to keep reaction temperature below ~50-60 °C. Cooling should be applied if the reaction becomes too violent.
   Q: The reaction from step 3 is mixed with either overhead stirrer or magnetic stirrer, combined with a cooler to keep the reaction mass under 60c temperature.
   
   
5. 1 L Of cooled distilled water is added to reaction mass, aluminum hydroxide is filtered off.
   Q: We add 1L of cold water into the reaction and use a buchner funnel with filter to clear it from aluminum residues?
   
   
6. The reaction mass extracted by DCM or petrolium ether 3 x 75 mL. Extracts are treated with 20 % HCl to pH 3. Resulting water layer from filtration is alkalinized by 20% NaOH aq to pH 12 and extracted with DCM or petrolium ether 3 x 75 mL. Organic layers with methamphetamine (4) are combined, concentrated in vacuum and dried over Na2SO4 or MgSO4 anhydrous.
   Q: I don't understand this at all, it's very unclear to me.
   
   I understand that there should be two different layers here. So I guess from step 5 when we add the cold water, and filter the reaction from residues of the aluminium. It will split into two layers. One organic and the one with water, the aqueous layer.
   
   The organic layer is extracted with DCM 3 x 75mL and then treated with 20% HCl to pH3
   
   The aqueous layer (water layer) is treated with with 20% NaoH to pH 12 and then extracted with DCM 3 x 75mL.
   
   After both layers are extracted and treated they are combined, concentrated in vacuum (optional) and dried using Na2SO4.
   
   If I am not wrong, this step is where we get our Methamphetamine freebase (Meth-oil)?
   
   
7. Preparation of methamphetamine hydrochloride is carried out by bubbling of dry HCl gas via organic layer. Precipitate is filtered off by suction filtration, dried. Also, you can grow Ice methamphetamine by following methods.
   Q: I don't understand this at all, it's very unclear to me.
   
   If I am not wrong, this is the step where we crystallize the Methamphetamine freebase (Meth-oil) to Methamphetamine?
   
   I would appreciate your input and knowledge on my question.
   
   Best Regards
   
   
   PS: Would admin please make this synthesis sticky.

ImOut1. You have to get amph free base (amph oil). You add 1 mole of salt to the solution of 20% aq NaOH ...
3. >81mL 37% aqueous formaldehyde and 350mL EtOH
They have to be already combined
4. +
5. +
6. >The organic layer is extracted with DCM 3 x 75mL and then treated with 20% HCl to pH3
You have to extract all mixture with DCM. After this extraction, you'll get aqueous layer, which have to be alkalized to pH 12 and extracted again. Then, both of these DCM extracts (which are contain Meth) have to be combined, dried over desiccant, and solvent is distilled off. You'll get methamph oil.

7. There are two options. First one, you buble HCl gas and get racemic amphetamine hydrochloride. Second one, you separate D-meth with l- or d-tartaric acid and get large shards of meth.

 

[G.Patton]

Hi everyone,

So it is time for me now to move forward in my progress and start looking at manufacturing Crystal Methamphetamine (ICE), I have no interest in "normal" Methamphetamines.

So let me start out with posting the step and asking my questions, I would appreciate any ones knowledgeable input.

Step:

1. You have to get 1 mole amphetamine free (1) base by addition salt of your amphetamine to 20% NaOH water solution to pH 12. Mix it for 15 min and extract amphetamine free base by DCM or petrolium ether 3 x 75 mL.
   Q: It says amphetamine free base, and then salt, does it mean freebase as in amphetamineoil or dry amphetamine, if I were to guess, it means amphetamine sulphate.
   
   
2. Prepare Al amalgam. You have to use approximately ~70 g of Al foil and 1.62 g mercury(II)nitrate (Hg(NO3)2) to make amalgam as described in following topic.
   Q: No question here
   
   
3. A mixture of 1 mole amphetamine freebase (136 g) and 1 mole aqueous formaldehyde (2) (81 mL 37% or 75 mL 40%) in 350 mL EtOH (ethanole) in 5 L round bottom flask with reflux condenser and an excess of aluminum amalgam, which was prepared in advance.
   Q: The extract from step 1 in is poured into a 5L round bottom flask, togheter with 81mL 37% aqueous formaldehyde and 350mL EtOH and the aluminium amalgam?
   
   
4. Imine (3) was reduced for approximately two hours, to keep reaction temperature below ~50-60 °C. Cooling should be applied if the reaction becomes too violent.
   Q: The reaction from step 3 is mixed with either overhead stirrer or magnetic stirrer, combined with a cooler to keep the reaction mass under 60c temperature.
   
   
5. 1 L Of cooled distilled water is added to reaction mass, aluminum hydroxide is filtered off.
   Q: We add 1L of cold water into the reaction and use a buchner funnel with filter to clear it from aluminum residues?
   
   
6. The reaction mass extracted by DCM or petrolium ether 3 x 75 mL. Extracts are treated with 20 % HCl to pH 3. Resulting water layer from filtration is alkalinized by 20% NaOH aq to pH 12 and extracted with DCM or petrolium ether 3 x 75 mL. Organic layers with methamphetamine (4) are combined, concentrated in vacuum and dried over Na2SO4 or MgSO4 anhydrous.
   Q: I don't understand this at all, it's very unclear to me.
   
   I understand that there should be two different layers here. So I guess from step 5 when we add the cold water, and filter the reaction from residues of the aluminium. It will split into two layers. One organic and the one with water, the aqueous layer.
   
   The organic layer is extracted with DCM 3 x 75mL and then treated with 20% HCl to pH3
   
   The aqueous layer (water layer) is treated with with 20% NaoH to pH 12 and then extracted with DCM 3 x 75mL.
   
   After both layers are extracted and treated they are combined, concentrated in vacuum (optional) and dried using Na2SO4.
   
   If I am not wrong, this step is where we get our Methamphetamine freebase (Meth-oil)?
   
   
7. Preparation of methamphetamine hydrochloride is carried out by bubbling of dry HCl gas via organic layer. Precipitate is filtered off by suction filtration, dried. Also, you can grow Ice methamphetamine by following methods.
   Q: I don't understand this at all, it's very unclear to me.
   
   If I am not wrong, this is the step where we crystallize the Methamphetamine freebase (Meth-oil) to Methamphetamine?
   
   I would appreciate your input and knowledge on my question.
   
   Best Regards
   
   
   PS: Would admin please make this synthesis sticky.

ImOutI'll clarify description.

 

[WinterDust]

Hi,

Followup question, step 2.

Can NaBH4 or LiAlH4 replace the Al/Hg?

If yes, what is the replacing weight for this synthesis, 70g?

Best regards

 

[G.Patton]

Hi,

Followup question, step 2.

Can NaBH4 or LiAlH4 replace the Al/Hg?

If yes, what is the replacing weight for this synthesis, 70g?

Best regards

ImOutI think yes, 1-1.2 molar excess is okay. Where did you take 70g?

Edit: I realized where did you take it.

 

[btcboss2022]

I think yes, 1-1.2 molar excess is okay. Where did you take 70g?

Edit: I realized where did you take it.

G.PattonI just doing it with the synth with 3 moles and 3.6 mols of NaBH4 replacing the amalgam and in cold atmosphere like others NaBH4 reductions at the moment seems ok tomorrow I will update the final result I left stirring now.
In point six I need to extract organic layer before treat it with HCl to PH3 and later basify the water layer to extract it?
Why first extraction is done before treat it to acid?And why make it acid if it's not extracted again?
Is not better basify all the mixture and extract once? Or if one part is better to extract it in acid should be done after treat it not before I guess no?
Strange process in point 6.
My formol 40% was in methanol solution in that case I don't need to dry it for NaBH4 reaction if your solution is with water you should dry it with sulfate if you want to use NaBH4 reduction.
Thanks.

 

[G.Patton]

I just doing it with the synth with 3 moles and 3.6 mols of NaBH4 replacing the amalgam and in cold atmosphere like others NaBH4 reductions at the moment seems ok tomorrow I will update the final result I left stirring now.
In point six I need to extract organic layer before treat it with HCl to PH3 and later basify the water layer to extract it?
Why first extraction is done before treat it to acid?And why make it acid if it's not extracted again?
Is not better basify all the mixture and extract once? Or if one part is better to extract it in acid should be done after treat it not before I guess no?
Strange process in point 6.
My formol 40% was in methanol solution in that case I don't need to dry it for NaBH4 reaction if your solution is with water you should dry it with sulfate if you want to use NaBH4 reduction.
Thanks.

btcboss2022Hi, sorry for a long reply.

In point six I need to extract organic layer before treat it with HCl to PH3 and later basify the water layer to extract it?

There is acid-base extraction: you have to make pH3, extract it. Then, make alkaline pH and extract it again. Extracts (organic layer) are combined.

Why first extraction is done before treat it to acid?And why make it acid if it's not extracted again?

what do you mean? This is typical acid-base extraction. You can read about theory of this procedure in my topic Extraction.

 

[JuanoImano4378]

1.62 g Mercury(II)nitrate (Hg(NO3)2);

G.PattonHey Patton, I can't get any anhydrous Mercury(II) nitrate where I'm from but I am able to get Mercury(II) nitrate monohydrate, (Hg(NO3)2).H2O. I read that in the aluminium amalgam summary that water is necessary. Does that mean the monohydrate version is possible to use?

 

[G.Patton]

Hey Patton, I can't get any anhydrous Mercury(II) nitrate where I'm from but I am able to get Mercury(II) nitrate monohydrate, (Hg(NO3)2).H2O. I read that in the aluminium amalgam summary that water is necessary. Does that mean the monohydrate version is possible to use?

JuanoImano4378Yes, affirmative. You have to recount an amount of Hg(NO3)2*H2O in accordance with molar ratio of Hg(NO3)2.

 

[JohnWebb]

Hello, can i use mercury ii chloride instead of nitrate?
Just approximately.. how much Meth can be made from 100g od Amph?

 

[UWe9o12jkied91d]

Hello, can i use mercury ii chloride instead of nitrate?
Just approximately.. how much Meth can be made from 100g od Amph?

JohnWebbyes, any mercury salt that is water soluble is fine
It has good yield, cant tell you exactly but its fine, over 50% for sure

 

[JohnWebb]

yes, any mercury salt that is water soluble is fine
It has good yield, cant tell you exactly but its fine, over 50% for sure

UWe9o12jkied91dGreat, thank you so much for responding

 

[nsrnsr]

I only have Paraformaldehyde, how to adjust the ratio of water solution? Thank you